Oxyfluorophosphate synthesis process and compound therefrom

Abstract

An electrolyte compound has the formula where p is an integer from 1 to 3 inclusive; and Y p+ is a metal ion, onium species, or proton; j is an integer value between 0 and 4 inclusive; k is an integer between 1 and 3 inclusive; and the sum 2k and j equals 6; Z is independently in each occurrence CR 1 R 2 or C(O); R 1 and R 2 are independently in each occurrence H, F or CH 3 . A process for preparing an oxyfluorophosphate is also provided.

1 . A process for preparing an oxyfluorophosphate comprising the step of:
 reacting a phosphorus pentafluoride complex with a metal alkoxy or an ester to liberate the heteroatom containing species.   
     
     
         2 . The process of claim  18  wherein said phosphorus pentafluoride complex is reacted with said metal alkoxy. 
     
     
         3 . The process of claim  18  wherein said phosphorus pentafluoride complex is reacted with said ester. 
     
     
         4 . The process of claim  19  wherein said metal alkoxy is a lithium oxalate. 
     
     
         5 . The process of claim  18  wherein said ester compound is a diester of a dicarboxylic acid. 
     
     
         6 . The process of claim  20  further comprising the step of exposing the oxyfluorophosphate to a halide under conditions suitable to create a halide salt thereof. 
     
     
         7 . The process of claim  22  wherein said dicarboxylic acid is oxalic acid. 
     
     
         8 . The process of claim  18  wherein said ester has a C 1 -C 8  alkyl ester group. 
     
     
         9 . The process of claim  19  wherein said metal alkoxy has the formula M 2 -O—R 1 —R 2 —R 3  where M 2  is an alkali metal, alkali earth, or quaternary ammonium cation; R 1  is C(O) or CR 4 R 5 ; R 2  is 
       
         
           
           
               
               
           
         
       
       R 3  is hydrogen, C(O)R 6 , CR 4 R 5 R 6 , or 
       
         
           
           
               
               
           
         
       
       where R 4  and R 5  are independently in each occurrence hydrogen, halogen, C 1 -C 8  alkyl, or C 0 -C 8  alkyl halogen; R 6  is hydrogen, OM 1 , SM 1 , or N(R 9 ) 2 ; where R 7  and R 8  are independently in each occurrence hydrogen, halogen, fluorine or C 1 -C 9  alkyl; where M′ is hydrogen, a 1+ valency metal ion, or a quaternary ammonium cation; where R 9  is independently in each occurrence is hydrogen, fluorine, or C 1 -C 8  alkyl; where X is a nullity, C 1 -C 8  alkyl, or C 1 -C 8  fluoroalkyl with the proviso that X is a nullity unless the pairs of R 4  and R 5 , or R 7  and R 8  are both carbon containing and together with X form a five or six member ring; and m is an integer from 0 to 6 inclusive. 
     
     
         10 . The process of claim  26  wherein R 3  is C(O)R 6  and R 6  is OM 1 . 
     
     
         11 . The process of claim  26  wherein R 3  is CR 4 R 5 R 6 , R 4  is fluorine, R 5  is fluorine and R 6  is OM 1 . 
     
     
         12 . The process of claim  19  wherein said metal alkoxy has the repeating unit formula: 
       
         
           
           
               
               
           
         
       
       where R 9  is independently in each occurrence a hydrogen, fluorine, or C 1 -C 8  alkyl; R 10  is a hydrogen, fluorine, OM 4 , or C 1 -C 8  alkyl; R 11  is C 0 -C 4  alkyl or C 6 -C 10  aryl; M 4  is hydrogen, a 1+ valency metal ion, C 1 -C 4  alkyl, or a quaternary ammonium cation; and M 3  is a 1+ valency metal ion. 
     
     
         13 . The process of claim  29  wherein R 9  is in each occurrence hydrogen. 
     
     
         14 . The process of claim  29  wherein R 10  is OM 4  and M 4  is lithium. 
     
     
         15 . The process of claim  29  wherein M 3  is lithium. 
     
     
         16 . The process of claim  18  further comprising the step of recrystallizing said oxyphosphate.